Process of making soap and detergent



UNITED STATES PAT N orrI-ce.

MAURICE AISEN, OF NEW YORK, N. YJAS SIGNOB TO GR AIN SOAPS CORPORATION, OF A DOVER, DELAWARE, A CORPORATION OF DELAWARE.

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No Drawing.

This invention relates to processes of making soap by means of hydrolyzing starches or proteids either by action of heat or by acid and heat combined, and treating the hydrolyzed product with caustic alkalis in a medium of anhydrous sodium or potassium carbonate, or any anhydrous salt of a similar chemical character.

Heretofore detergent compounds have been made from cereals, whlch are a mixture of starches (carbo-hydrates), proteins (nitrogenous matter) and glycerids of fatty acids (fats). These substances have been treated either individually, or in mixture with comparatively strong solutions of alkalis (caustic soda or caustic potash). In the case of starches or roteids the resulting combination. createdi sodium orpotassium salts of starches or proteids which are of a complex nature with a high molecular structure. The cereals used have been mostly corn, oats, wheat and rice, which are heavy in starches and are built up from a number of simpler compounds of low molec ular structure, polymerized in nature to a compound of high molecular structure.

In my improved process, I do not use cereals as such, but, first, by hydrolysis of the starches and proteids, I break down their high molecular structure into compounds of the same chemical family but of as each simplier compound will fix an alkali,

and, by weight, will combine with more alkali; (3) the simpler compounds have a more active acid groupment, that is, the alkali being stronger combined, will hydrolyze slower and be less likely to affect fab- Speciflcatlon of Letters Patent.

Application filed November 20 1919. Serial No. 889,406.

rics injuriously in washing; (4) the hydrolyzed simpler compounds are very active surface colloids, with great penetrability, and are quickly soluble in waten.

The theory of washing by means of alkalifatty acids, especially those of sodium salts of fatty acids, is that when this compounds is dissolved in water it hydrolyzes. The acid salts of the fatty acids are colloids of great surface activity and penetrability, whlch separate and unloosen dlrt and grease mechanically attached to the material to be washed, and the free sodium hydroxid chemically combines with the grease and the dirt. The acid salts of the fatty acid emulslfies these new formed sodium compounds which are soluble to a lar e extent in water; by rinsing both the solu les and insolubles are removed.

vThe alkali-cereal compounds heretofore used, when hydrolyzed in water for washing purposes, revert back practically to their ori 'inal alkali and starch. The starch, while a colloid, has little, or practically no, surface activity or washing efficacy, and the efficiency of such alkali-cereal compound is practically entirely dependent upon the efficacy of the alkali contents of the compounds. The hydrolyzed simplified cereal compounds, utilized by my process, are very active surface colloids and also are quickly soluble in water, and therefore add greatl to the' penetrability and efficacy of the prod not of my invention as a washing agent.

When an alkali is combined with the hydrolyzed simpler compounds of starches and proteids, the action is very violent; this is because these hydrolyzed simpler compounds are much more chemically active than the complex compounds of the starch and proteids. Because the action of the alkali on the simpler hydrolyzed compounds is so violent and since it would not be economical to use diluted alkali solutions, it becomes essential to utilize some medium to reduce the violence of the chemical action and stop further conversion before carbonization when "alkalizing the simpler hydrolyzed compounds with strona'alkali solutions. For this purpose, I have found that anhydrous' sodium carbonate, or anhydrous potassium carbonate, or any anhydrous salt of similar character, is well suited to produce the desired effect; these salts will reduce the violence of the chemical action. Other means of a similar character may be used without departing from my invention. The water of the caustic alkali solution is absorbed by the anhydrous salt. Then by raising the temperature of the mass to the melting point of the carbonate, now hydrated, saponification of the hydrolyzed mass takes place. 1

My process may be clearly understood by the following illustrations: The cereal (say 250 pounds) is heated, preferably in a steam jacketed drier, from'one and one-half to four hours at a high temperature but below the carbonization temperature (the carbonization temperature is substantially 180 centigrade), the mass being constantly stirred during the heating. By this treatment'the cereal is hydrolyzed to compounds of simpler, or lower, molecular structure having a stronger acid nature than the original cereal. The higher the temperature (but below the carbonization temperature) the shorter the time it will take to hydrolyze the cereal. The change of color, from yellow to brown, indicates when the desired chemical change has been accomplished. To this hydrolyzed product I add anhydrous sodium carbonate (substantially 100 pounds) which has the effect of stopping any further conversion.

When the mass has cooled, I spray into the hydrolyzed sodium carbonate mixture caustic soda (substantially 45 to 55 pounds of 98% strength according to degree of hydrolyzation) which has been dissolved in water (in substantially 135 pounds). The anhydrous sodium carbonate, being very avid for its water of crystallization, absorbs the greater part of the moisture, leaving a very intimately mixed product, slightly alkalined, of the hydrolyzed cereal, sodium carbonate crystals and practically dry caustic soda.

The temperature of the mass is then gradually raised to the melting point of the sodium carbonate crystals (below 100 centigrade) and maintained at such temperature for substantially one hour, at which time all the cereal will have been alkalined.

Then all the sodium carbonate crystals may be neutralized with a substantially equivalent amount of fatty acid, the amount of fatty acid used depending upon the nature of the fatty acid. The product is an efficient detergent compound.

Substantially the same result can be accomplished by a slight modification of the above illustration, as for example: Into the cereal (say 250 pounds) is sprayed a dilute form (substantially 0.1 to 0.25%, figured at 100%) of hydrochloric acid, or nitric acid (substantially two pounds); then heating the mixture three-quarters to one and onehalf hours at a temperature substantially between 150 .and 160 degrees centigra de: the time and temperature can be determined by the change in color of the mixture from yellow to brown, depending upon the amount of hydrolyzed action desired. To this mixture add anhydrous sodium carbonate (substantially 100 pounds).'- When the .mass is cooled, add. caustic soda dissolved in water and then subject-to heat to the melting point of the sodium carbonate crystals, substantially as in the previous illustration.

By another slight modification the same result is accomplished,'viz: The cereal (say 250 pounds) is hydrolyzed either as in the first or second. illustration above, and when hydrolyzed anhydrous sodium carbonate (substantially 100 ounds) is added. To this mixture add atty acids sufiicient to emulsify and. neutralize the sodium carbonate (100 to 200 pounds, depending upon the nature of the acid). This mixture is dry and the sodium carbonate will produce no chemical action, or practically none, except that it emulsifies the fatty acids and incorporates in the emulsion the hydrolzed cereal. Dissolve caustic soda (substantially 45 to 55 pounds according to degree of hydrolyzation) in water (in substantially 125 pounds) and add to the emulsified mass a sufficient amount of this caustic soda solution to complete the saponification of the fatty acid, the quantity depending upon the nature of the fatty acid. In this modification the anhydrous sodium carbonate may be omitted, for the reason that the fatty acid will prevent a too violent chemical reaction of the alkali and hydrolyzed cereal,

By still another modification the same result is accomplished, viz: To anhydrous sodium carbonate (say 100 lbs.) saturated with its water of crystallization from a solution of caustic soda add hydrolyzed cereal (substantially 250 lbs), raise the temperature of the mass to the melting point of the sodium carbonate crystals (below 100 centigrade) and the mass will saponify, and free caustic will be substantially absent; if a fatty acid soap is desired as a part of the mixture in the final product, add to the hydrolyzed cereal after it has been mixed with the saturated sodium carbonate a fatty acid as desired and a sufiicient quantity of the solution of caustic soda to saponify the fatty acid used.

The cereals used are preferably the flour of corn, oats, wheat, rice, etc., but any substance rich in starch may be employed.

In stating the order of mixing the ingredients. the proportions of the different ingredients and the strength of the acids and alkalis used, it must be understood that I do not limit myself to the above stated proportions of the ingredients, or the order of their mixture, or the quantity or strength of the .acids and alkalis employed; good results may be obtained under my process by a considerable variance from the proportions and strength of the ingredients used. Nor do I limit myself to the'stated chemical agents used as, as is well known to chemists, other chemical agents may be substituted to produce the same results. The ingredients and chemical agents above stated, however, I have found, in practice, to be efficient, economical and productive of a high grade detergent.

Subject matter disclosed in this specification which is not here claimed is claimed in concurrent ending applications, Ser. No. 413,907, filed Sept. 30, 1920, Ser. No. 415,272 filed Oct. 7, 1920, and Ser. No. 413,761, filed Sept. 30, 1920.

I claim:

1. The

rocess of makin soap from cereals conslsting in hydrolyzmg the cereal bysubjecting same to a high temperature, but below" the carbonization temperature which is substantially 180 centigrade, for substantially two hours; to this hydrolyzed mass adding anhydrous sodium carbonate in the proportion by weight substantially of one part of sodium carbonate to two and onealf parts of cereal; spraying into the mixture substantially one-seventh by weight of caustic soda dissolved in water; raising the temperature of the mass to the melting point of the sodium carbonate crystals (below 100 centigrade) andmaintaining at such temperature for substantially one hour; and finally neutralizing any free sodium carbonate crystals and caustic soda with a fatty acid.

2. The process of making soap from cereals consisting in hydrolyzing the cereal by subjecting same to a high temperature for substantially two hours and saponifying the hydrolyzed mass by caustic soda in a me (hum of sodium carbonate crystals.

3. The process of making soap from cereals consisting in hydrolyzin the cereal and saponifying the hydrolyze mass by an alkali.

4. The process of making soap from cereals consisting in hydrol zing the cereal and saponifying the hydro yzed mass by an alkali in a medium of sodium-carbonate crystals, or equivalent alkali metal carbonate or stals.

y MAURICE AISEN. Witnesses FRANKLIN A. WAGNER,

F. A. SPAETH. 

